a. Field of Invention
The invention relates generally to a system and a methodology for controlling multifunctional multireactor chemical synthesis instruments. The invention system and methodology employ real time automatic controls, calculations, feedbacks and optional graphic tracking of parameters, process characteristics, events and offer templates for designing otherwise complex sequences for the bench chemist, physicist or biologist. Automatic lab notebook construction is also provided as well as remote monitoring and control options, warning alarms and shut down alarms.
b. Description of Related Art
The following patents are representative of prior art related to various types of heated/cooled reaction vessels:
U.S. Pat. No. 2,472,362 to Herbert L Barnebey et al. describes a method of successively heating and cooling the contents of a vessel by means of a fluid medium, the steps of confining a body of vaporizable fluid in a hermetically sealed space about the bottom and sides of a vessel to be heated defined by the vessel wall and an auxiliary condensing surface, maintaining a portion of said fluid body in the liquid state as a pool contacting the bottom of said vessel, first applying extraneous heat to boil the liquid and heat the vessel and its contents by exchange of heat through the vessel walls from the hot liquid and condensing vapors, then ceasing to apply extraneous heat to the liquid, and finally extraneously cooling said auxiliary condensing surface causing the vessel and its contents to cool by boiling the liquid pool in contact with said vessel bottom, and condensing the resulting vapor on said surface.
U.S. Pat. No. 2,739,221 to G. H. Morey describes a vessel heater as recited in claim 2 wherein said means includes a first valve communicating with a supply of non-inflammable and non-combustion-supporting fluid in its gaseous phase to regulate admission of a quantity of fluid to blanket said heating element and thereby preclude ignition of combustible products adjacent said heating element, and a second valve communicating with a supply of non-inflammable and non-combustion-supporting fluid in its liquid phase to regulate admission of a quantity of fluid to effect rapid cooling of the vessel.
U.S. Pat. No. 2,894,881 to Clinton M. Wolston, Jr. et al. describes a laboratory distillation testing apparatus having a condenser tank, a flask, a flask supporting means, a heating means, a condenser tube passing through the said tank, and a light diffusing panel, the improvements which comprise a recess in said condenser tank, a shield means disposed within said recess, adjustable shelf means carried by said shield means for supporting said flask, conduit means below said tank, and solenoid valve means on said conduit means, the discharge end of said conduit means projecting forwardly of the rear wall of said recess below said condenser tube inlet and arranged to discharge forwardly and downwardly towards said shelf means.
U.S. Pat. No. 3,143,167 to A. Vieth describes a temperature controlled enclosure comprising a first metal wall surrounding the enclosure space, a heating means in thermal contact with said first wall for raising the temperature of the enclosure, a second metal wall surrounding the heating means, cooling means in thermal contact with said second wall for lowering the temperature of the enclosure, a first temperature-sensitive element in thermal contact with said first metal wall, a second temperature-sensitive element in thermal contact with said second metal wall, and a control circuit connected between said elements and said heating and cooling means for energizing the heating and cooling means selectively to produce a desired temperature within the enclosure, said control circuit including a bridge, an amplifier, and a switching means for connecting the heating means to a source of power when said first temperature-sensitive element is connected to the bridge and for activating the cooling means when said second temperature-sensitive element is connected to the bridge.
U.S. Pat. No. 3,239,432 to Joseph C. Rhodes et al. describes an apparatus for controlling the operation of a first distillation column and for determining the distillation properties of a product sample from said first column which apparatus comprises: means for withdrawing a product sample containing a mixture of liquids having different boiling points from said first column; a test column member; a plurality of liquid-retaining trays spaced apart vertically within said test column; a liquid sample container positioned below said test column and in flow communication with the bottom-most portion of said test column; means for receiving said withdrawn product sample and introducing a known amount of said product sample into said container; means for vaporizing liquid sample introduced into said container; vapor riser means for passing vapors from the lower portion of said test column upwardly through said test column to intimately contact liquid retained on said trays; condensing means communicating with the upper end of said test column to condense all the vapors rising from the upper-most of said trays; means for returning the resulting condensate to the upper-most of said trays; means for maintaining the test column pressure at a substantially constant pressure during a run; means for maintaining a pre-selected level of liquid on said trays; temperature sensing means to sense the temperatures and produce a temperature signal indicative thereof of equilibrium vapors above the trays in said test column; means for receiving said temperature signal and correlating the sensed temperatures with the distillation properties of a known product sample of approximately the same composition as said sample being run and produced an output signal relative to said correlation; and means for receiving said output signal and adjusting the control parameters of the first column in accordance with said output signal.
U.S. Pat. No. 3,473,387 to Charles Meriam describes an inclined-manometer-type of fluid characteristic measuring instrument which is responsive to pressure sensing for directly reading volume, weight or velocity of flow, or differential pressure across a flow measuring orifice, nozzle, venturi or laminar flow element or for directly reading static head, velocity head or total head fluid pressure. Adjustments are provided for correcting the instrument reading measurements for variations in fluid measurement conditions, including temperature of, density of, viscosity of, barometric pressure on, humidity of, mixture of fluids in, etc. of the fluid being measured; temperature, etc. of the manometer liquid; etc.
U.S. Pat. No. 3,479,252 to Kurt Anders Holm et al. describes an invention which is concerned with an apparatus for degreasing articles by means of a boiling solvent or vapor originating therefrom. The apparatus has double walls, and cooling means which are provided between said double walls. The cooling means comprise water spraying means, and means for passing ventilation air through the space defined by said double walls. Consequently, the ventilation air has the double function of withdrawing solvent vapor and cooling the wall of the apparatus.
U.S. Pat. No. 4,019,365 to Lecon Woo describes a thermomechanical analyzer adapted to measure stress or strain in a sample material by the use of a flat, passive spring, having a known modulus of elasticity, in conjunction with an axially displaceable shaft which mechanically links the spring and the sample together. The linkage is such that the sample under test and the spring are mechanically connected in parallel, i.e., each undergo equal displacement. A transducer senses axial displacement of the shaft such that the magnitude of the shaft displacement is related to the stress in the sample. The sample may be subjected to temperature variations during the test cycle.
U.S. Pat. No. 4,030,314 to John Frederick Strehler describes preservation of biological materials accomplished by apparatus and a process with and by which the material is cooled at a substantially linear rate to approximately freezing temperature, changed from the liquid to the solid phase at relatively constant temperature, and cooled at a substantially linear rate to and end temperature. The environment surrounding the material is rapidly chilled when the material reaches freezing temperature or a temperature minimally warmer than freezing temperature in the liquid phase to initiate phase change with minimal risk of super cooling the material, and is then warmed to freezing temperature or a temperature minimally cooler than freezing temperature to minimize temperature drop in the material upon completion of phase change. The apparatus contemplates, among other things, preselection of cooling rates, duration of phase change, and the end temperature.
U.S. Pat. No. 4,043,762 to George Milton Olds describes a coupling means for test tubes and the like, the coupling means enabling the coupling of test tubes to other objects or devices for various purposes, as for example, support purposes. In one embodiment of the invention, the coupling means is comprised of a flexible, resilient, tubular body portion which is open at each end and which is adapted to be slideably circumimposed on a portion of the periphery of a conventional tubular test tube of the type that is closed at one end, the coupling means also including a pair of circumferentially spaced, flexible, resilient and integral flange portions which project longitudinally outwardly from one end of the tubular body portion and which define openings adjacent the free ends thereof adapted to receive a cooperating member such as the stem of a conventional funnel, a support rod, a thermometer or other object to which it is desired to couple a test tube. In another embodiment of the invention, the coupling means is formed integrally with the body portion of a test tube.
U.S. Pat. No. 4,117,881 to Thomas E. Williams et al. describes blood cells, blood marrow, and other similar biological tissue that is frozen while in a polyethylene bag placed in abutting relationship against opposed walls of a pair of heaters. The bag and tissue are cooled with refrigerating gas at a time programmed rate at least equal to the maximum cooling rate needed at any time during the freezing process. The temperature of the bag, and hence of the tissue, is compared with a time programmed desired value for the tissue temperature to derive an error indication. The heater is activated in response to the error indication so that the temperature of the tissue follows the desired value for the time programmed tissue temperature. The tissue is heated to compensate for excessive cooling of the tissue as a result of the cooling by the refrigerating gas. In response to the error signal, the heater is deactivated while the latent heat of fusion is being removed from the tissue while the tissue is changing phase from liquid to solid.
U.S. Pat. No. 4,276,264 to Jury V. Redikultsev et al. describes a device for sterilizing water-containing liquid media by steam which comprises a sterilizing vessel with inlet and outlet connections for processed liquid media. A heater is provided in the lower portion of the vessel, while a condenser is arranged in the upper portion thereof. The vessel also houses a coaxially mounted steam-transfer unit representing gas-lift tube with a diffuser disposed over the heater.
U.S. Pat. No. 4,346,754 to Leland A. Imig et al. describes a heating and cooling apparatus capable of cyclic heating and cooling of a test specimen undergoing fatigue testing. Cryogenic fluid is passed through a block 10 clamped to the specimen 11 to cool the block and the specimen. Heating cartridges 13 penetrate the block 10 to heat the block and the specimen 11 to very hot temperatures. Control apparatus 36 and 46 is provided to alternately activate the cooling and heating modes to effect cyclic heating and cooling between very hot and very cold temperatures. The block 10 is constructed of minimal mass to facilitate the rapid temperature change thereof.
U.S. Pat. No. 4,480,682 to Hiroshi Kaneta et al. describes an apparatus for freezing fertilized ova, spermatozoa or the like has a heat transfer bottom board block formed at the lower end of a heat insulating peripheral wall with a lower refrigerant passage capable of flowing refrigerant. A bottom board temperature sensor is attached to the bottom board block, an upper heat transfer block is placed on the bottom board block through a heat insulating joint member, formed with an upper refrigerant passage for flowing the refrigerant. A temperature control heater, an upper block temperature sensor, a plurality of erecting tube charging spaces of tubes opened at the top thereof with the bottom gourd block as a bottom member are disposed between the peripheral wall and the upper block in such a manner that the tubes erected and charged into the spaces are cooled at the lower ends thereof by said bottom board block and at the upper part containing articles to be frozen such as fertilized ova, spermatozoa or the like are contained in buffer solution in said tubes. Thus, the buffer solutions in the tubes can be controlled to be cooled at the buffer solution of the lower noncontaining part by the bottom board block and the buffer solution of the containing part above the buffer solution of the lower noncontaining part by the upper block.
U.S. Pat. No. 4,489,569 to Helmuth Sitte describes a cooling apparatus utilizing liquid nitrogen for cooling specimens to temperatures in the range from −100° C. to −195° C. in propane, halogenated hydrocarbons, isopentane, or other cooling media. Freezing of the cooling media is avoided by means of an arrangement wherein the liquid nitrogen cools the cooling-bath container and/or the liquifier only initially, but after the desired cooling-bath temperature has been reached, the liquid nitrogen level is lowered to below the height of a protective shell which results in further cooling being only indirect, via solid/solid contacts and via the gas phase. A constant cooling-bath temperature is ensured by means of a thermostatic temperature-control system while trouble-free standby operation is ensured by means of an automatic system for replenishing liquid nitrogen, and by a system for controlling the level of liquid nitrogen. Safe disposal of the cooling media which may be combustible and/or toxic is provided for.
U.S. Pat. No. 4,502,531 to Peter Petersen describes an invention that provides an apparatus and method or heating a vessel having a vessel bottom and at least one vessel side wall. The invention includes a furnace housing which is adapted to contain the vessel and which has a housing bottom and at least one housing side wall. A heater mechanism, located at the housing bottom and at the housing side wall, heats the vessel and is adapted to contact selected portions of the vessel bottom and vessel side wall. Thermal insulation is disposed about the housing for reducing heat loss therefrom, and an extendable temperature sensor is adapted to contact the vessel and monitor the temperature thereof.
U.S. Pat. No. 4,548,259 to Sadao Tezuka describes a flow cell for containing sample solutions is surrounded by an electric heater which is then surrounded by an isothermal frame having a large heat capacity, and a Peltier element serving as a cooling source is coupled with the isothermal frame. A heat delaying plate is arranged between the flowcell and heater and a temperature sensor is arranged between the flowcell and the heat delaying plate. The Peltier element is controlled in such a manner that the temperature of the isothermal frame is maintained substantially at a constant temperature lower than a predetermined temperature at which the sample solution is to be kept. The heater is controlled in accordance with a difference between the temperature of the sample solution and the predetermined temperature.
U.S. Pat. No. 4,563,883 to Hellmuth Sitte describes a device for immersing a specimen into a cryogenic cooling liquid comprising an injector for carrying a specimen, means for accelerating the injector to a predetermined velocity vertically into the liquid, and means for rotating the injector, before the vertical movement ends, or at moment it ends, to promote heat transfer from the specimen. Various means for effecting rotation of the injector are described.
U.S. Pat. No. 4,578,963 to Hellmuth Sitte describes an apparatus for the cryofixation of specimens, comprises a tank adapted to contain a cold gaseous medium having an upper boundary with an atmosphere external to the tank, and cooling means having an upper surface, said cooling means being disposed within the tank. The upper surface is movable between a lower level and an upper level which is below the upper boundary. The upper surface is maintained at the upper level for a period sufficient to permit the application of a specimen to the upper surface, and is then lowered to the tower level.
U.S. Pat. No. 4,667,730 to Georg Zemp describes a temperature regulating apparatus for a laboratory reaction vessel arrangement, which comprises a reaction vessel and a thermal chamber for a fluid heat exchange medium which at least partially surrounds the reaction vessel. A jacketing vessel is provided with at least one inlet aperture for said fluid heat exchange medium and at least partially surrounds the thermal chamber. The at least one inlet aperture is arranged to extend through the jacketing vessel and into the thermal chamber, and a nozzle is arranged in a region of the at least one inlet aperture. This nozzle has an outlet orifice and is arranged in the region of the at least one inlet aperture such that the fluid heat exchange medium flows through the nozzle and out of the outlet orifice and such that the fluid heat exchange medium flowing out of the outlet orifice subsequently flows into said thermal chamber.
U.S. Pat. No. 4,846,257 to Terry A. Wallace et al. describes an apparatus for keeping food hot and/or cold which includes a body of heavily insulated material in which there are separate recesses for hot food and cold food. The cold food is kept cold by means of an ice compartment located in the bottom recess and an exhaustible refrigeration unit located in the top of that recess. The hot food is kept warm by means of an electrical coil in the bottom of the recess and a solar heating panel in the top.
U.S. Pat. No. 4,966,469 to Douglas S. Fraser et al. describes a positioning device for a temperature sensor in a flask for freeze drying. The device comprises a generally circular plastic stopper having an opening approximately in its center. The stopper is snap-fittingly secured to the top of the flask. A central, annular tube extends through that opening and into the flask. A thermocouple having a generally circular cross section is coiled around and supported by the annular tube so that it is free and is in the center of the flask. The thermocouple is retractable and extensible to permit the use of the thermocouple in flasks of various lengths.
U.S. Pat. No. 5,123,477 to Jonathan M. Tyler describes a thermal reactor, and a method of operating the thermal reactor, in which the thermal reactor includes a chamber which is thermally isolated by refrigerated air circulating in the walls of the chamber, and which holds a tray of sample vials, means for supplying air to the chamber and for exhausting air from the chamber; heaters for heating the air supplied to the chamber; sensors for sensing the temperature of the air supplied to the chamber and of the sample vials, and a computer which pulses the heaters according to the measured temperatures of the vials and the air in the chamber to maintain the temperature of the vials at a desired level.
U.S. Pat. No. 5,139,079 to Michael L. Becraft describes a present invention providing for improved performance of a dynamic mechanical analyzer which measures mechanical and rheological properties of a material by reducing thermal lag in the material by modifying the radiative oven thereof to include a convective transfer device.
U.S. Pat. No. 5,154,067 to Takeshi Tomizawa describes a portable cooler for cooling an article by utilizing the endothermic and exothermic phenomenon pertaining to a chemical reaction which is disclosed, in which an adsorbent and a working medium are sealed in a reaction chamber defined between an inner wall and an outer wall, a working medium retaining member which is disposed on the inner wall inside the reaction chamber for holding therein the working medium, the working medium retaining member being spaced from the adsorbent disposed on the outer wall, and a heater is held in contact with the adsorbent for regenerating the same, at least a part of said outer wall constituting a heat radiating portion.
U.S. Pat. No. 5,171,538 to Ewald Tremmel et al. describes a reagent supply system for a medical analytical instrument which includes a reagent space provided on the instrument and reagent vessels which are received in the reagent space. In the reagent space there is provided at least one reagent vessel compartment with a bottom, lateral guide elements, and a top guiding element, as well as a front stop. The instrument contains a fluid communication system for connection with a reagent vessel situated in the reagent vessel compartment. On the end face of the reagent vessel compartment is disposed a hollow needle near the bottom surface thereof and extending in a direction which is parallel to the bottom surface. The reagent vessel has on its front wall facing the end face a pierceable seal with pierceable elastic stopper.
U.S. Pat. No. 5,176,202 to Daniel D. Richard describes a method used in low temperature storage of biological specimens comprising the steps of (a) maintaining a multiplicity of biological specimens within a predetermined low temperature range in a cryogenic storage unit, (b) selecting at least one biological specimen for removal from the storage unit, (c) determining a respective thaw period and thaw rate for the selected specimen, (d) automatically retrieving the selected specimen from the storage unit at removal time in accordance with the respective determined thaw period, and (e) automatically thawing the selected specimen at the respective thaw rate. An associated thawing system comprises a storage unit for maintaining a plurality of biological specimens within a predetermined low temperature range, a plurality of thawing chambers, and a heat exchange assembly for implementing a temperature change in each of the chambers independently of temperature changes in the other chambers. A servomechanism is provided for retrieving selected specimens from the storage unit and transferring the retrieved specimens to respective thawing chambers, while a control unit is operatively connected to the heat exchange assembly and the servomechanism for operating the heat exchange assembly to control rates of temperature changes in the thawing chambers and for activating the servomechanism to transfer the selected specimens from the storage unit to the respective chambers.
U.S. Pat. No. 5,203,203 to William L. Bryan et al. describes an apparatus for measuring in situ the viscosity of a fluid in a sealed container which includes a spherical ball forming an integral package before any fluid is placed within the container. The apparatus further includes a composite ball consisting of a spherical core of one material surrounded by one or more layers of different materials distributed spherically about the core. The container may also be supported by an angular support member which angularly positions the container such that the ball will move within the container through the fluid at specific speed. A sensing device is provided along the wall of the container to measure the speed of the ball wherein the sensing device includes a pair of sensors spaced apart by a known distance to sense when the ball passes by each of the sensors providing a speed which is useful for calculating the viscosity of the fluid.
U.S. Pat. No. 5,337,806 to Josef Trunner describes a bath in which the supply reservoir is arranged for the liquid, in which the reaction flask to be heated or cooled can be immersed. The heating or cooling device is arranged on the bottom of the supply reservoir. The liquid is delivered with an immersion pump through a feed pipe and an opening in the bottom of the bath. The level of the liquid in the bath can be adjusted with the aid of a slider. The liquid flows back into the supply reservoir over an overflow. When the pump is switched off, the liquid in the bath flows independently back into the supply reservoir.
U.S. Pat. No. 5,447,374 to Douglas S. Fraser et al. describes a method and device for positioning a probe, such as a temperature sensor, in a flask. A stopper adapted to be secured to an open end of the flask is provided having an opening through which a tube extends. A clamping mechanism is connected to the tube to secure the probe to the stopper. The clamping mechanism comprises a first flange, and a second opposing flange spaced slightly apart from the first flange. An O-ring positioned around the flanges causes them to flex inward to engage and secure the probe between them.
U.S. Pat. No. 5,489,532 to Stanley E. Charm describes an automatic test apparatus for use in a test method to determine antimicrobial drugs. The test apparatus comprises a first aluminum, electrically heatable block with holes for the insertion of test containers and a separate, second cooling aluminum block adapted to be placed periodically in contact with the heated aluminum block to cool rapidly the heated block. The test apparatus includes timed signals existing therein to alert the test user. The test apparatus is adapted to provide for the timed sequential solid heating and cooling of one or more test containers containing a test sample.
U.S. Pat. No. 5,689,895 to David T. Sutherland et al. describes a device for positioning a probe, such as a temperature sensor, in a flask for freeze drying. The device includes a stopper adapted to be secured to an open end of the flask. The stopper has a center opening and at least one radial opening spaced from the center opening. The radial opening allows for fluid communication between inside and outside of the flask when the stopper is secured to the open end of the flask. The center opening receives a guide tube which extends into the flask and is sized to receive the probe such that substantially no fluid communication between the inside of the flask and the outside of the flask occurs through the guide tube or center opening. A channel formed in an upper surface of the stopper and the O-ring positioned about an outer diameter of a neck of the flask secure the probe in position relative to the guide tube. The multiple radial openings define an annular passageway which mimics fluid communication through a standard slit-type stopper employed in freeze drying.
U.S. Pat. No. 5,947,343 to Klaus Horstmann describes a flask for liquids, in particular an insulating flask, in which a pouring aperture can be closed by a lid which can be releasably attached to the flask. The lid is provided with a closure element which can be moved by a handle and is loaded by a spring element towards a closed position. The closure element is movable in a substantially vertical opening motion between an open position, in which the pouring aperture is released, and the closed position, in which the pouring aperture is closed. In order to ensure that the closure element is movable by an uncomplicated, durable mechanism, with the pouring aperture being easily openable and effectively closable during operation, the spring element is formed from a spring-elastic diaphragm connection the closure element to the lid.
U.S. Pat. No. 6,095,356 to Miriam Rits describes a vented flask cap having a body portion with proximal and distal ends with a generally cylindrical sidewall extending from the proximal end to the distal end of first and second support plates are formed at the proximal end of the body portion and having a plurality of apertures extending there-through; a filter assembly is also provided which includes a first, lower membrane having a first porosity, a second, upper membrane having a second porosity and a radiation absorbing material disposed between the first and second membranes.
U.S. Pat. No. 6,502,456 B1 to Yaosheng Chen describes a method and an apparatus that are disclosed for the measurement of the aridity, temperature, flow rate, total pressure, still pressure, and kinetic pressure of steam at a downhole location within a well through which wet steam is flowing. The apparatus comprises a series of fiber optic sensors that are mounted on sections of a shell assembly. The apparatus is lowered into a well to different downhole locations, and measures the multiple parameters of steam at different locations and heights. The data can be stored on board for subsequent analysis at the surface when the apparatus is retrieved from the well. The apparatus is very reliable, accurate, and of long-life in harsh environments.
U.S. Pat. No. 6,615,914 to Li Young describes a reaction vessel system that includes a reaction vessel, a cooling unit functionally connected to the vessel to impart controlled cooling thereto; a heating unit functionally connected to the vessel to impart controlled heating thereto; and control means connected to the cooling unit and the heating unit for programmable automatic control of the cooling unit to control at least one of the on/off flow and rate of flow, and to control at least one of on/off heating and rate of heating, including a programmable device. The cooling unit includes a cooling element in proximity to the vessel with at least one inlet port for injection of a phase change coolant, a heat absorbent area and at least one outlet port for removal of the phase change coolant. This is an injector for injecting the coolant in liquid form via the inlet port to the cooling element. In preferred embodiments, the control means includes software, and the system includes an injection physical control device, for cyclical on/off control thereof to establish a predetermined temperature sequence involving a plurality of diverse, programmable temperature levels. The phase change coolant used in the present invention is an environmentally inert material which absorbs heat upon vaporization and has a boiling point below room temperature at atmospheric pressure, and may be selected from the group consisting of inert gases, carbon dioxide, and nitrogen.
European Patent No. EP 0 400 965 A2 to Kondo Akihiro describes a reagent reactor comprising a vial having an opening at one end thereof; a supporting block, having a first heater element, for surrounding and supporting said vial in a substantially erected position so that said opening of the vial is adjacent to the upper surface thereof and exposed to the outside thereabove; a cover block pressing against said supporting block under pressure and capable of sealing said opening of said vial including a fluid introducing tube projecting from said operating into said vial when the cover block is in the sealing position to the vial, a fluid discharging opening opposed to said opening when the cover block is in the sealing position to the vial, and a second heater element; and a temperature control circuit for controlling said first and second hater elements so as to maintain the temperature of the upper portion of aid vial and the lower end surface of said cover block which contacts said opening of said vial more than the temperature of the main body of said vial when a reagent is added to a sample contained in said vial so as to allow reaction of the reagent with said sample and when the evaporation or the azeotropy of a reagent or a solvent is performed.
Notwithstanding the prior art, the present invention is neither taught nor rendered obvious thereby.